ORGLIST: Making Isocyanate thro' Triphosgene

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From: mailbox (mailbox$##$invalid)
Date: Sun Mar 06 2005 - 00:41:23 EST


Hello Friends !

I'm trying a lot to perform a reaction of making an aliphatic Isocyanate =
from its Amine or its Hydrochloride salt. But unfortunately not being =
succeeded. Using molar ratio as Amine/Amine HCl : Triphosgene : =
TEA/DIPEA as 1 : 0.4 : 2.0 in toluene & maintaining temperature at =
reflux & in another experiments the temperature at 70 deg C. The time of =
reaction I tried from 2 hours to 8 hours. But after the reaction, the =
TLC & the GC report still shows a large amount of Amine/Amine HCl =
unconverted. Only 20-25% of Amine is being converted to the Isocyanate.

Can anyone pls give me some advice or some experimental data to complete =
this reaction ?



Thanking you all in advance,
Kamal




   



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